[go: up one dir, main page]

ATE163441T1 - APPLYING A FLUOROPOLYMER FILM TO A BODY - Google Patents

APPLYING A FLUOROPOLYMER FILM TO A BODY

Info

Publication number
ATE163441T1
ATE163441T1 AT92913016T AT92913016T ATE163441T1 AT E163441 T1 ATE163441 T1 AT E163441T1 AT 92913016 T AT92913016 T AT 92913016T AT 92913016 T AT92913016 T AT 92913016T AT E163441 T1 ATE163441 T1 AT E163441T1
Authority
AT
Austria
Prior art keywords
pct
film
applying
fluoropolymer film
sec
Prior art date
Application number
AT92913016T
Other languages
German (de)
Inventor
Thomas Ronald Thomas
Original Assignee
British Tech Group
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by British Tech Group filed Critical British Tech Group
Application granted granted Critical
Publication of ATE163441T1 publication Critical patent/ATE163441T1/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • C08J7/123—Treatment by wave energy or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12—Composite membranes; Ultra-thin membranes
    • B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
    • B01D69/127—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction using electrical discharge or plasma-polymerisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06—Organic material
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • B01D71/36—Polytetrafluoroethene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/62—Plasma-deposition of organic layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/14—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by electrical means
    • B05D3/141—Plasma treatment
    • B05D3/142—Pretreatment
    • B05D3/144—Pretreatment of polymeric substrates
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • D06M10/025—Corona discharge or low temperature plasma
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08—Organic compounds
    • D06M10/10—Macromolecular compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
    • D06M14/18—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation
    • D06M14/26—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin
    • D06M14/30—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials using wave energy or particle radiation on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M14/34—Polyamides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
    • D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/16—Sizing or water-repelling agents
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
    • D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
    • D21H23/22—Addition to the formed paper
    • D21H23/32—Addition to the formed paper by contacting paper with an excess of material, e.g. from a reservoir or in a manner necessitating removal of applied excess material from the paper
    • D21H23/42—Paper being at least partly surrounded by the material on both sides
    • D21H23/44—Treatment with a gas or vapour
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
    • D21H25/04—Physical treatment, e.g. heating, irradiating
    • D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/22—Polymers or copolymers of halogenated mono-olefins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2400/00—Specific information on the treatment or the process itself not provided in D06M23/00-D06M23/18
    • D06M2400/01—Creating covalent bondings between the treating agent and the fibre
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03—Non-macromolecular organic compounds
    • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/11—Halides

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Textile Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Laminated Bodies (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

PCT No. PCT/GB92/01111 Sec. 371 Date Apr. 26, 1994 Sec. 102(e) Date Apr. 26, 1994 PCT Filed Jun. 19, 1992 PCT Pub. No. WO93/00394 PCT Pub. Date Jul. 1, 1993.A thin fluoropolymer film is covalently bonded to a microporous ptfe film to make a bilayer for separation, filtration or reverse osmosis, by exposing the microporous film to perfluorocyclohexane under plasma.
AT92913016T 1991-06-20 1992-06-19 APPLYING A FLUOROPOLYMER FILM TO A BODY ATE163441T1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB919113350A GB9113350D0 (en) 1991-06-20 1991-06-20 Asymmetric/anisotropic fluoropolymer membrane manufacture

Publications (1)

Publication Number Publication Date
ATE163441T1 true ATE163441T1 (en) 1998-03-15

Family

ID=10697031

Family Applications (1)

Application Number Title Priority Date Filing Date
AT92913016T ATE163441T1 (en) 1991-06-20 1992-06-19 APPLYING A FLUOROPOLYMER FILM TO A BODY

Country Status (12)

Country Link
US (1) US5516561A (en)
EP (1) EP0590007B1 (en)
JP (1) JP3356776B2 (en)
AT (1) ATE163441T1 (en)
AU (1) AU665004B2 (en)
CA (1) CA2111852C (en)
DE (1) DE69224523T2 (en)
DK (1) DK0590007T3 (en)
ES (1) ES2113429T3 (en)
GB (1) GB9113350D0 (en)
HK (1) HK1014015A1 (en)
WO (1) WO1993000394A1 (en)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5773098A (en) * 1991-06-20 1998-06-30 British Technology Group, Ltd. Applying a fluoropolymer film to a body
EP1088567B1 (en) * 1998-02-23 2008-12-03 Bespak plc Drug delivery devices
EP1448807A4 (en) * 2001-10-30 2005-07-13 Massachusetts Inst Technology FLUOROCARBON-ORGANOSILICIUM COPOLYMERS AND COATINGS PREPARED BY CHEMICAL VAPOR DEPOSITION BY HOT FILAMENT
WO2004041397A2 (en) * 2002-05-09 2004-05-21 Massachusetts Institute Of Technology Preparation of asymmetric membranes using hot-filament chemical vapor deposition
KR101194646B1 (en) 2005-12-30 2012-10-24 엘지디스플레이 주식회사 Fabricating method of soft mold
GB0713821D0 (en) * 2007-07-17 2007-08-29 P2I Ltd A plasma deposition apparatus
GB0721527D0 (en) * 2007-11-02 2007-12-12 P2I Ltd Filtration Membranes
WO2011090717A1 (en) * 2009-12-28 2011-07-28 Gvd Corporation Coating methods, systems, and related articles
US9475105B2 (en) * 2010-11-08 2016-10-25 University Of Florida Research Foundation, Inc. Articles having superhydrophobic and oleophobic surfaces
US8852693B2 (en) 2011-05-19 2014-10-07 Liquipel Ip Llc Coated electronic devices and associated methods

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3700489A (en) * 1970-07-30 1972-10-24 Ethicon Inc Process for applying a thin coating of polytetrafluoroethylene
US4391843A (en) * 1981-08-14 1983-07-05 Rca Corporation Adherent perfluorinated layers
DE3214804A1 (en) * 1982-04-21 1983-10-27 Siemens AG, 1000 Berlin und 8000 München METHOD FOR PRODUCING A LYOPHOBIC LAYER
DE3326377A1 (en) * 1983-07-22 1985-01-31 Siemens AG, 1000 Berlin und 8000 München METHOD FOR PRODUCING GLIMP POLYMERISATE LAYERS
JPS6197008A (en) * 1984-10-17 1986-05-15 Mitsubishi Chem Ind Ltd Thin film manufacturing method
US5091204A (en) * 1985-08-23 1992-02-25 Weshington Research Foundation Polymeric intraocular lens material having improved surface properties
US4869922A (en) * 1986-01-24 1989-09-26 Ausimont S.P.A. Method of coating with polyfluorocarbons
GB8613015D0 (en) * 1986-05-29 1986-07-02 Thomas T R Porous ptfe
IT1215418B (en) * 1987-04-10 1990-02-08 Ausimont Spa PERFLUOROALKANS OBTAINED BY PHOTOCHEMICAL FLUORURATION AND THEIR USE AS POLYMERIZATION INITIATORS.
US5094895A (en) * 1989-04-28 1992-03-10 Branca Phillip A Composite, porous diaphragm
JP2990608B2 (en) * 1989-12-13 1999-12-13 株式会社ブリヂストン Surface treatment method
US5331454A (en) * 1990-11-13 1994-07-19 Texas Instruments Incorporated Low reset voltage process for DMD
US5246451A (en) * 1991-04-30 1993-09-21 Medtronic, Inc. Vascular prosthesis and method
US5244730A (en) * 1991-04-30 1993-09-14 International Business Machines Corporation Plasma deposition of fluorocarbon
US5387378A (en) * 1993-04-21 1995-02-07 Tulane University Integral asymmetric fluoropolymer pervaporation membranes and method of making the same

Also Published As

Publication number Publication date
DK0590007T3 (en) 1998-03-16
CA2111852C (en) 2004-08-31
AU2020892A (en) 1993-01-25
US5516561A (en) 1996-05-14
ES2113429T3 (en) 1998-05-01
JPH06508648A (en) 1994-09-29
JP3356776B2 (en) 2002-12-16
WO1993000394A1 (en) 1993-01-07
HK1014015A1 (en) 1999-09-17
CA2111852A1 (en) 1993-01-07
DE69224523D1 (en) 1998-04-02
GB9113350D0 (en) 1991-08-07
DE69224523T2 (en) 1998-07-02
EP0590007A1 (en) 1994-04-06
EP0590007B1 (en) 1998-02-25
AU665004B2 (en) 1995-12-14

Similar Documents

Publication Publication Date Title
DE69217529D1 (en) Membrane gas separation process
DE69224523D1 (en) APPLYING A FLUOROPOLYMER FILM TO A BODY
TR28306A (en) Liquid replaceable quilted faced film laminates.
ZA916032B (en) Multilayer reverse osmosis membrane of polyamide-urea
DE68914774D1 (en) Multi-layer microporous film laminates.
DE3852414D1 (en) Composite membranes for the separation of fluids.
AU588817B2 (en) Multilayer reverse osmosis membrane in which one layer is poly-meta-phenylene cyclohexane-1,3,5-tricarboxamide
SE9501369D0 (en) Multiple filter unit
FR2676007B1 (en) COMPOSITE NANOFILTRATION MEMBRANE.
DE3886053D1 (en) Body fluid filter with permeable flat film membranes that have protruding parts.
ATE181878T1 (en) MULTI-LAYER POLYURETHANE FILM AND USE THEREOF FOR PRODUCING PACKAGING FOR PHOTO-SENSITIVE MATERIAL
DE69132554D1 (en) New multi-component fluid separation membrane
DE3886057D1 (en) Reverse osmosis membranes.
ATE78422T1 (en) PLUGGED MICROPOROUS FILM.
ITTO910327A1 (en) PERMSELECTIVE MEMBRANES AND THEIR USE
FR2678177B1 (en) INORGANIC MEMBRANE FOR FILTRATION AND, FILTER UNIT OBTAINED.
AU4685889A (en) Process for separating organometallic compounds and/or metal carbonyls from their solutions in organic media
DE59100594D1 (en) Dispenser for the operation of double cartridges.
DE59200926D1 (en) Membrane couplings with perforated contour membranes.
ATE164094T1 (en) FILTER ARRANGEMENT
DE58906606D1 (en) Optically active rhodium complexes of 3,4-bis (diarylphosphino) pyrrolidines and their use for the preparation of phosphinothricin by asymmetric hydrogenation.
FR2676394B1 (en) BACKED DOCUMENT MEDIUM, IN PARTICULAR CONSTITUTING A PERSONALIZED POSTCARD.
DE59300046D1 (en) Drinking water treatment device.
JPS56107424A (en) Multilayer flexible thin film switch
ATE157254T1 (en) DEXTRINE DERIVATIVES AND THEIR USE IN THE TREATMENT OF POISONING

Legal Events

Date Code Title Description
UEP Publication of translation of european patent specification
REN Ceased due to non-payment of the annual fee